CN103553051A - Method for separating solids from liquid of dregs in production process of organic silicon - Google Patents
Method for separating solids from liquid of dregs in production process of organic silicon Download PDFInfo
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- CN103553051A CN103553051A CN201310520607.8A CN201310520607A CN103553051A CN 103553051 A CN103553051 A CN 103553051A CN 201310520607 A CN201310520607 A CN 201310520607A CN 103553051 A CN103553051 A CN 103553051A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention belongs to the field of chemical engineering, and particularly relates to a method for separating solids from liquid of dregs in the production process of organic silicon. According to the technical scheme aiming at the technical problem, the method comprises the steps of: adding a bulking agent into dregs according to the mass ratio of dregs to bulking agent being 1:0.5-1:0.01, stirring, then distilling, collecting high-boiling dregs, and adding hydrolyte into the distilled solids so that the distilled solids are fully hydrolyzed. The method overcomes the problems that the remaining distilled solids are difficult to discharge, and the treatment process in the technology is simple and easy to operate, the high-boiling dregs of the organic silicon can be recycled, so that the cost can be lowered, and the environment pollution can also be reduced.
Description
Technical field
The invention belongs to chemical field, be specifically related to the method for screenings solid-liquid separation in a kind of organic silicon production process.
Background technology
Screenings (hereinafter to be referred as screenings) in organosilicon production, due to a kind of liquid-solid mixture with mobility that adopts wet dedusting to obtain in methyl chlorosilane monomer building-up process, screenings is processed to adopt and at the temperature of 200 ℃ of left and right, is carried out flash distillation, solid-liquid ratio 3 ︰ 7 left and right of screenings after discharging, liquid phase in screenings after flash distillation is mainly organosilicon high-boiling product, solid phase is mainly suspension silica flour, high-content copper and other metal, if this part material is exposed in air, will burn and form strong acid liquid contamination environment.Therefore the screenings after flash distillation need to be distilled again, after most high boiling material is distilled away, then be hydrolyzed.But due in still-process, along with high boiling material constantly reduces, solids is easy to caking, causes discharging difficulty.The object of this invention is to provide a kind of easy-operating method, improves after screenings solid-liquid separation, and solids is difficult for the problem of discharging.
Summary of the invention
The object of the invention is to reclaim a large amount of organosilicon high-boiling products by underpressure distillation, the residual organosilicon high-boiling product in remaining solids is hydrolyzed, overcome hydrolysis in former technique and not exclusively, caused the solids after hydrolysis to contain the problems such as organosilicon high-boiling product; Add raising agent simultaneously, overcome the problem of remaining solid thing discharging difficulty after distillation.
Technical problem to be solved by this invention is to provide the method for screenings solid-liquid separation in a kind of organic silicon production process.The method comprises the following steps:
A, Jiang Zha ︰ raising agent=1 ︰ 0.5～1 ︰ 0.01 in mass ratio, add raising agent in screenings, stirs; Wherein, described raising agent is at least one in silicone oil, calcium carbonate, sodium carbonate or silicon-dioxide;
B, by the mixture distillation of step a, collect cut, be organosilicon high-boiling product;
C, the screenings after distillation is joined to be no less than account for after distillation in the hydrolyzed solution of screenings 50wt%, fully hydrolysis, filters, and collects solids; Described hydrolyzed solution is at least one in water, calcium carbonate aqueous solution or aqueous sodium carbonate.
Concrete, the screenings described in above-mentioned separation method step a is for carrying out the liquid-solid mixture with mobility of the wet dedusting step gained in methyl chlorosilane monomer building-up process the screenings of flash distillation gained.
Concrete, described in above-mentioned separation method step a, churning time is 0.5～3h.
Concrete, the distillation condition described in above-mentioned separation method step b is 120～160 ℃ of temperature, vacuum tightness-0.04～-0.1Mpa.
Concrete, the distillation time described in above-mentioned separation method step b is 1～6h.
Concrete, in the calcium carbonate aqueous solution described in above-mentioned separation method step c, the massfraction of calcium carbonate is 5～50%.
Concrete, in the aqueous sodium carbonate described in above-mentioned separation method step c, the massfraction of sodium carbonate is 1～40%.
Concrete, hydrolyzed solution described in above-mentioned separation method step c accounts for 50～150wt% of the rear screenings of distillation.
Concrete, the mode that adds described in above-mentioned separation method step c is to add while stirring screenings.
The present invention also provides the solids obtaining by above-mentioned separation method step c.
The inventive method process treatment process is simple, easy to operate.Meanwhile, the present invention has added raising agent before underpressure distillation, has improved the sponginess of screenings gained solids after distillation, has overcome the problem of remaining solid thing discharging difficulty after distillation; After liquid filtering after hydrolysis, can reuse again as hydrating solution, the solids after filtration can be brought as carrying copper raw material, has not only realized utilization of waste material, has also reduced the pollution to environment simultaneously simultaneously.
Embodiment
A method for screenings solid-liquid separation in organic silicon production process, comprises the following steps:
A, Jiang Zha ︰ raising agent=1 ︰ 0.5～1 ︰ 0.01 in mass ratio, add raising agent in screenings, stirs 0.5～3h; Wherein, described raising agent is at least one in silicone oil, calcium carbonate, sodium carbonate or silicon-dioxide;
B, mixed organic silicon slurry slag is joined in still kettle, under 120～160 ℃, vacuum tightness-0.04～-0.1Mpa, distill 1～6h, collect cut, obtain organosilicon high-boiling product;
C, the screenings after distillation is joined to be no less than account for after distillation in the hydrolyzed solution of screenings 50wt%, fully hydrolysis, filters, and collects solids; Described hydrolyzed solution is at least one in water, calcium carbonate aqueous solution or aqueous sodium carbonate.
The solids finally obtaining by the inventive method, wherein copper content is 3～10wt%, silica flour content is 40～60wt%.
For organosilicon high-boiling product remaining in screenings after distillation being reacted away, the present invention has added water, calcium carbonate aqueous solution or aqueous sodium carbonate to realize this object; In order to improve the sponginess of screenings gained solids after distillation, overcome the problem of remaining solid thing discharging difficulty after distillation, separation method of the present invention has added raising agent before underpressure distillation.
The inventive method is processed rear solid phase prod can carry copper, brickmaking, cement processed etc.; After processing, the high boiling material of gained can again enter wet method dedusting system or carry out producing of high boiling point silicon oil simultaneously; Thereby the organosilicon high-boiling product that the inventive method is separating obtained and solids, can carry out next step recycling, not only saved cost, reduced environmental pollution simultaneously.
Embodiment 1
By the organic silicon slurry slag of 100 weight parts (wherein cupric, silica flour, high boiling material etc., solid-to-liquid ratio=3 ︰ 7), add 10 weight part calcium carbonate, stir 0.5h, be warmed up to 130 ℃, start vacuum system, condenser system, control vacuum tightness for-0.08Mpa is distilled to and distillates without high boiling material, stop vacuum system, condenser system, collection high boiling material is 30 parts; Distillation test residue is joined to 100 parts, concentration again and be in 1wt% sodium carbonate solution after fully hydrolysis, filter, collect solids, in this solids, copper content is 3.5%, and silica flour is 45.8%.
Embodiment 2
By the organic silicon slurry slag of 100 weight parts (wherein cupric, silica flour, high boiling material etc., solid-to-liquid ratio=3 ︰ 7), add 50 weight part sodium carbonate, stir 1h, be warmed up to 150 ℃, start vacuum system, condenser system, control vacuum degree control for-0.07Mpa is distilled to and distills out without high boiling material, stop vacuum system, condenser system, collection high boiling material is 30 parts; The solids after distillation is joined to 80 parts, concentration again and be in 40wt% calcium carbonate soln after fully hydrolysis, filter, collect solids, in this solids, copper content is 3.9%, and silica flour is 47%.
Embodiment 3
By the organic silicon slurry slag of 100 weight parts (wherein cupric, silica flour, high boiling material etc., solid-to-liquid ratio=3 ︰ 7), add 20 weight part sodium carbonate, stir 1h, be warmed up to 140 ℃, start vacuum system, condenser system, control vacuum degree control for-0.07Mpa is distilled to and distills out without high boiling material, stop vacuum system, condenser system, collection high boiling material is 30 parts; The solids after distillation is joined in 80 parts after fully hydrolysis again, filter, collect solids, in this solids, copper content is 3.8%, and silica flour is 46.8%.
Embodiment 4
By the organic silicon slurry slag of 100 weight parts (wherein cupric, silica flour, high boiling material etc., solid-to-liquid ratio=3 ︰ 7), add 30 weight part silicon-dioxide, stir 1h, be warmed up to 140 ℃, start vacuum system, condenser system, control vacuum degree control for-0.07Mpa is distilled to and distills out without high boiling material, stop vacuum system, condenser system, collection high boiling material is 30 parts; The solids after distillation is joined to 80 parts, concentration again and be in 40wt% calcium carbonate soln after fully hydrolysis, filter, collect solids, in this solids, copper content is 4%, and silica flour is 49.3%.
Reference examples 1
By the organic silicon slurry slag of 100 weight parts (wherein cupric, silica flour, high boiling material etc., solid-to-liquid ratio=3 ︰ 7), open and stir, be warmed up to 140 ℃, start vacuum system, condenser system, control vacuum degree control is-0.07Mpa, along with distilling out of high boiling material, solids in screenings condenses into piece gradually, the hardness of the solids of caking increases gradually, even if also cannot make the solids of caking disperse under the effect of stirring, in discharging, the solids of these cakings just goes out to stop up discharge port like this.
Result contrast: can be found out by reference examples 1, if do not add raising agent before distillation, outflow along with high boiling material, in screenings, solids condenses into piece gradually, and the hardness of the solids of caking increases gradually, even if also cannot make the solids of caking disperse under the effect of stirring, in discharging, the solids of these cakings just goes out to stop up discharge port like this, thereby discharging is difficult, can not carry out further work simultaneously, wasted human and material resources; Yet the present invention has added raising agent before distillation, although also can lump in distillation, but the hardness of this caking solids is very little, very loose, under the effect of stirring, will well disperse, thereby discharging is easy, not only can saves human and material resources, and can save time, make equipment can continue in a short period of time to use, obtained unforeseeable technique effect.
Claims (10)
1. a method for screenings solid-liquid separation in organic silicon production process, is characterized in that: comprise the following steps:
A, Jiang Zha ︰ raising agent=1 ︰ 0.5～1 ︰ 0.01 in mass ratio, add raising agent in screenings, stirs; Wherein, described raising agent is at least one in silicone oil, calcium carbonate, sodium carbonate or silicon-dioxide;
B, by the mixture distillation of step a, collect cut, be organosilicon high-boiling product;
C, the screenings after distillation is joined in the hydrolyzed solution that is no less than the screenings 50wt% accounting for after distillation, fully hydrolysis, filters, and obtains solids; Described hydrolyzed solution is at least one in water, calcium carbonate aqueous solution or aqueous sodium carbonate.
2. method according to claim 1, is characterized in that: in step a, described screenings is for carrying out the liquid-solid mixture with mobility of the wet dedusting step gained in methyl chlorosilane monomer building-up process the screenings of flash distillation gained.
3. method according to claim 1, is characterized in that: in step a, described churning time is 0.5～3h.
4. method according to claim 1, is characterized in that: in step b, described distillation condition is 120～160 ℃ of temperature, vacuum tightness-0.04～-0.1Mpa.
5. method according to claim 1, is characterized in that: in step b, described distillation time is 1～6h.
6. method according to claim 1, is characterized in that: in step c, in described calcium carbonate aqueous solution, the massfraction of calcium carbonate is 5～50%.
7. method according to claim 1, is characterized in that: in step c, in described aqueous sodium carbonate, the massfraction of sodium carbonate is 1～40%.
8. method according to claim 1, is characterized in that: in step c, described hydrolyzed solution accounts for 50～150wt% of the rear screenings of distillation.
9. method according to claim 1, is characterized in that: in step c, the described mode that adds is to add while stirring screenings.
10. the solids obtaining in claim 1～9 any one method steps c.
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| CN201310520607.8A CN103553051B (en) | 2013-10-29 | 2013-10-29 | Method for separating solids from liquid of dregs in production process of organic silicon |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045059A (en) * | 2014-06-25 | 2014-09-17 | 泸州北方化学工业有限公司 | Organosilicon slurry slag hydrolysis treatment process, byproduct and application thereof |
| CN104129823A (en) * | 2014-07-14 | 2014-11-05 | 江苏三鼎水处理设备有限公司 | High-precision silicon-removing device |
| CN109260815A (en) * | 2018-09-26 | 2019-01-25 | 褚成亮 | A kind of organosilicon slag slurry processing method |
| CN112707930A (en) * | 2021-01-04 | 2021-04-27 | 江西蓝星星火有机硅有限公司 | Method for recovering high-boiling-point substances in organic silicon slurry slag |
| CN114292288A (en) * | 2021-12-13 | 2022-04-08 | 华陆工程科技有限责任公司 | Method for treating synthetic reaction slurry in production of methyl silicate by directly synthesizing silicon powder |
| CN114524408A (en) * | 2022-02-14 | 2022-05-24 | 浙江大学 | Environment-friendly comprehensive recycling method of organic silicon pulp residues |
Citations (4)
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|---|---|---|---|---|
| US4221691A (en) * | 1979-02-16 | 1980-09-09 | Dow Corning Corporation | Method of hydrolyzing chlorosilanes |
| CN1618840A (en) * | 2003-11-21 | 2005-05-25 | 中国石油天然气股份有限公司 | Method for treating organic silicon waste residue slurry |
| CN101386626A (en) * | 2008-10-31 | 2009-03-18 | 江苏宏达新材料股份有限公司 | Organosilicon slag slurry treatment method and apparatus thereof |
| CN102180605A (en) * | 2010-12-27 | 2011-09-14 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Process for treating organic silicon slurry slag |
-
2013
- 2013-10-29 CN CN201310520607.8A patent/CN103553051B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4221691A (en) * | 1979-02-16 | 1980-09-09 | Dow Corning Corporation | Method of hydrolyzing chlorosilanes |
| CN1618840A (en) * | 2003-11-21 | 2005-05-25 | 中国石油天然气股份有限公司 | Method for treating organic silicon waste residue slurry |
| CN101386626A (en) * | 2008-10-31 | 2009-03-18 | 江苏宏达新材料股份有限公司 | Organosilicon slag slurry treatment method and apparatus thereof |
| CN102180605A (en) * | 2010-12-27 | 2011-09-14 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Process for treating organic silicon slurry slag |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045059A (en) * | 2014-06-25 | 2014-09-17 | 泸州北方化学工业有限公司 | Organosilicon slurry slag hydrolysis treatment process, byproduct and application thereof |
| CN104045059B (en) * | 2014-06-25 | 2016-08-24 | 泸州北方化学工业有限公司 | Organic silicon slurry slag hydrolysis process technique and by-product and application thereof |
| CN104129823A (en) * | 2014-07-14 | 2014-11-05 | 江苏三鼎水处理设备有限公司 | High-precision silicon-removing device |
| CN104129823B (en) * | 2014-07-14 | 2015-08-05 | 常州三鼎环保科技有限公司 | High precision silica removal equipment |
| CN109260815A (en) * | 2018-09-26 | 2019-01-25 | 褚成亮 | A kind of organosilicon slag slurry processing method |
| CN112707930A (en) * | 2021-01-04 | 2021-04-27 | 江西蓝星星火有机硅有限公司 | Method for recovering high-boiling-point substances in organic silicon slurry slag |
| CN114292288A (en) * | 2021-12-13 | 2022-04-08 | 华陆工程科技有限责任公司 | Method for treating synthetic reaction slurry in production of methyl silicate by directly synthesizing silicon powder |
| CN114524408A (en) * | 2022-02-14 | 2022-05-24 | 浙江大学 | Environment-friendly comprehensive recycling method of organic silicon pulp residues |
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